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CN1942398B - Seeded boehmite particulate material and methods for forming same - Google Patents

Seeded boehmite particulate material and methods for forming same Download PDF

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CN1942398B
CN1942398B CN 200580011124 CN200580011124A CN1942398B CN 1942398 B CN1942398 B CN 1942398B CN 200580011124 CN200580011124 CN 200580011124 CN 200580011124 A CN200580011124 A CN 200580011124A CN 1942398 B CN1942398 B CN 1942398B
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boehmite
material
particulate
precursor
suspension
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CN 200580011124
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Chinese (zh)
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CN1942398A (en )
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D·叶纳
M·巴恩斯
M·斯科隆
R·鲍尔
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圣戈本陶瓷及塑料股份有限公司
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; MISCELLANEOUS COMPOSITIONS; MISCELLANEOUS APPLICATIONS OF MATERIALS
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/02Emulsion paints including aerosols
    • C09D5/024Emulsion paints including aerosols characterised by the additives
    • C09D5/028Pigments; Filters
    • C09D7/43
    • C09D7/70

Abstract

A boehmite particulate material is disclosed. The material is formed by a process that includes providing a boehmite precursor and boehmite seeds in a suspension, and heat treating the suspension to convert the boehmite precursor into boehmite particulate material. The boehmite particulate material has an aspect ratio of not less than 3:1.

Description

引晶勃姆石微粒材料及其形成方法 Seeded boehmite particulate material and methods of forming

[0001] 相关申请的交叉引用 CROSS [0001] REFERENCE TO RELATED APPLICATIONS

[0002] 本申请是:(i)于2003年4月16日提交的美国专利申请10/414590的部分继续申请,10/414590又是于2002年4月19日提交的美国临时申请60/374014的非临时申请; 和(ii)于2004年4月13日提交的美国专利申请10/823400的部分继续申请。 [0002] This application is: US Patent (i), 2003 April 16 part 10/414590 filed a continuation application US 10 / 414,590 is on April 19, 2002, filed provisional application 60/374014 non-provisional application; the US Patent and (ii) in 2004 April 13 part 10/823400 filed a continuation application. 本申请要求上述申请的优先权,其主题内容通过参考结合于此。 This application claims priority of the above application, the subject matter of which is incorporated herein by reference.

[0003] 背景 [0003] BACKGROUND

发明领域 Field of the Invention

[0004] 本申请一般地涉及勃姆石微粒材料和形成该材料的方法。 [0004] The present application generally relates to boehmite particulate material and the method of forming the material. 本发明更具体地涉及具有形态特征的引晶(seeded)勃姆石微粒材料。 The present invention relates more particularly to seeded (seeded) having morphological characteristics boehmite particulate material.

[0005] 相关技术说明 [0005] Description of Related Art

[0006] 勃姆石微粒材料特别可用作形成含铝产品如高性能氧化铝磨料粒的原料。 [0006] In particular boehmite particulate material may be used as raw material to form an aluminum-containing products such as high performance alumina abrasive grains. 在此背景下,属本受让人共有的美国专利4797139中揭示了形成勃姆石微粒材料的具体方法,该材料随后可用作后续加工形成氧化铝磨料粒的阶段的进料。 In this context, the case of common assignee of the present U.S. Patent No. 4,797,139 discloses a specific method for forming boehmite particulate material, the material is subsequently used as a feed stage subsequent processing to form alumina abrasive grains. 如文中所述,勃姆石材料通过引晶处理的方法(seeded process)形成,并且局限于勃姆石微粒材料适应形成氧化铝磨料粒的范围内。 As described herein, the boehmite material is formed by a method (seeded process) seeded process, and limited to the boehmite particulate material adapted to form alumina abrasive grains in a range. 因此,所揭示的微粒材料具有特别期望的球形形态,这种形态使得它适用于研磨应用。 Thus, the particulate material is disclosed having a particular desired spherical morphology, this form makes it suitable for abrasive applications.

[0007] 除了研磨应用外,特别需要产生各种不同形态的勃姆石微粒材料。 [0007] In addition to grinding applications, particularly desirable to produce various forms of boehmite particulate materials. 因为微粒形态可对材料的应用产生深远的影响,所以本领域中对于产生除磨料之外的新应用材料的需求不断增加,包括用于专用涂料产品和各种聚合物产品的填料。 Since particulate morphology can have a profound impact on the application material, the present art for the generation of a new application of an abrasive material other than increasing demand, comprising a filler dedicated for coating products and various polymer products. 其它应用包括其中勃姆石材料就以其形成时的状态而不是作为进料使用的那些应用。 Other applications include those in which the boehmite material is formed on it in the state of the application rather than those used as feed. 人们除了对产生新材料感兴趣外,能够形成这种材料的加工技术也必需加以开发。 In addition to the processing techniques to produce people interested in the new materials, but can be formed of such materials must also be developed. 就此而言,这种加工技术要有令人满意的投入产出、可直截了当的加以控制、并且能够提供高产率。 In this regard, such processing technology have satisfactory input and output, can be controlled straightforward, and can provide high yields.

[0008] MM [0008] MM

[0009] 依据一个方面,通过引晶处理形成的勃姆石微粒材料的纵横比不小于3 : 1。 [0009] According to one aspect, the aspect of the boehmite particulate material formed by seeded processing is not less than 3: 1.

[0010] 依据本发明的另一个方面,勃姆石微粒材料通过包括以下步骤的方法形成:以悬浮液的形式提供勃姆石前体和勃姆石晶种,对该悬浮液进行加热处理,以使勃姆石前体转化成勃姆石微粒材料。 [0010] According to another aspect of the present invention, boehmite particulate material formed by a process comprising the steps of: providing a boehmite precursor and boehmite seeds in a suspension, the suspension is subjected to heat treatment, so that the boehmite precursor into boehmite particulate material. 该微粒材料可以具有一定的形态,例如较高的纵横比,例如不小于约2 : 1,例如不小于约3 : 1。 The particulate material may have a certain morphology, such as higher aspect ratios, such as not less than about 2: 1, such as not less than about 3: 1.

[0011] 另外,依据本发明的另一个方面,勃姆石微粒材料通过包括以下步骤的方法形成: 以悬浮液的形式提供勃姆石前体和勃姆石晶种,对该悬浮液进行加热处理,以使勃姆石前体转化成勃姆石微粒材料。 [0011] Further, according to another aspect of the present invention, boehmite particulate material formed by a process comprising the steps of: providing a boehmite precursor and boehmite seeds in a suspension, heating the suspension process, so that the boehmite precursor into boehmite particulate material. 此处,勃姆石微粒材料由薄片组成,其纵横比不小于约2 : 1,例如不小于约3 : 1。 Here, the boehmite particulate material composed of a sheet, an aspect ratio of not less than about 2: 1, such as not less than about 3: 1.

[0012] 附图简要说明 [0012] BRIEF DESCRIPTION OF DRAWINGS

[0013] 图1是说明片形勃姆石微粒材料的SEM显微照片。 [0013] FIG. 1 is a SEM micrograph stone sheet-shaped boehmite particulate material.

[0014] 图2是说明针形勃姆石微粒材料的SEM显微照片。 [0014] FIG 2 is a SEM micrograph of a needle-shaped boehmite particulate material. [0015] 图3是说明椭球形勃姆石微粒材料的SEM显微照片。 [0015] FIG. 3 is a SEM micrograph stone ellipsoidal boehmite particulate material.

[0016] 图4是说明球形勃姆石微粒材料的SEM显微照片。 [0016] FIG. 4 is a SEM micrograph of spherical boehmite particulate material.

[0017] 优选实施方式的说明 DESCRIPTION [0017] The preferred embodiment

[0018] 依据本发明的一个实施方式,勃姆石微粒材料通过包括以下步骤的方法形成:以悬浮液的形式提供勃姆石前体和勃姆石晶种,加热(例如,通过热液处理)该悬浮液(或者溶胶或浆料),使勃姆石前体转化成颗粒或微晶形成的勃姆石微粒材料。 [0018] According to an embodiment of the present invention, boehmite particulate material formed by a process comprising the steps of: providing a boehmite precursor and boehmite seeds in a suspension, heating (e.g., by hydrothermal treatment ) the suspension (alternatively sol or slurry), boehmite precursor into particles or microcrystalline boehmite particulate material formed. 依据一具体方面, 所述勃姆石微粒材料具有相对细长的形态,在文中一般用下文所述的纵横比来描述。 According to one particular aspect, the boehmite particulate material has a relatively elongated morphology, described generally by the following description of the aspect ratio.

[0019] 文中一般使用的术语“勃姆石”指水合氧化铝,包括:矿物勃姆石,通常为A1203 • H20,含水量约为15% ;以及假勃姆石(psuedoboehmite),含水量高于15重量%,例如20-38重量%。 [0019] generally used herein the term "boehmite" refers to hydrated alumina, comprising: mineral boehmite, typically A1203 • H20, moisture content of about 15%; and pseudo-boehmite (psuedoboehmite), high water content to 15 wt%, e.g. 20-38 wt%. 要指出的是,勃姆石(包括假勃姆石)具有特定且可确认的晶体结构, 因而也具有独特的X射线图谱,并且因此有别于其它含铝材料,包括其它水合氧化铝,例如ATH(三水合氧化铝),它是这里用于制造勃姆石微粒材料的一种常规前体材料。 It is noted that boehmite (including pseudo-boehmite) having a specific and identifiable crystal structure, and thus has a unique X-ray pattern, and therefore is different from other aluminous materials including other hydrated aluminas, e.g. ATH (alumina trihydrate), which is used herein for manufacturing a precursor material of a conventional boehmite particulate material.

[0020] 纵横比定义为最长尺寸与垂直于该最长尺寸的第二长尺寸的比值,一般不小于2 : 1,优选不小于3 : 1、4 : 1或6 : 1。 [0020] The aspect ratio is defined as the ratio of the second longest dimension to the long dimension perpendicular to the longest dimension, is generally not less than 2: 1, preferably not less than 3: 1, 4: 1 or 6: 1. 事实上,某些实施方式具有相对细长的颗粒,例如不小于9 : 1,10 : 1,在某些情况下,不小于14 : 1。 Indeed, certain embodiments have relatively elongated particles, such as not less than 9: 1, 10: 1, in some cases, not less than 14: 1. 特别涉及针形颗粒,颗粒可进一步用第二纵横比来表征,第二纵横比定义为第二最长尺寸与第三最长尺寸的比例。 In particular, relates to needle-shaped particles, the particles may be further characterized by a second aspect ratio, the aspect ratio of the second second longest dimension to the third longest dimension is defined as the ratio. 第二纵横比一般不大于3 : 1,通常不大于2 : 1,或者甚至1.5 : 1,时常约为1 : 1。 The second aspect ratio is generally not greater than 3: 1, typically not greater than 2: 1, or even 1.5: 1, often about 1: 1. 第二纵横比一般描述颗粒在垂直于最长尺寸的平面内截面几何形态。 Secondary aspect ratio generally describes the particle-sectional geometry in a plane perpendicular to the longest dimension.

[0021] 板形或片形颗粒一般具有细长结构,具有以上结合针形颗粒所描述的纵横比。 [0021] The plate-shaped or sheet-shaped particles generally have an elongated structure having the aspect ratios described above in connection needle-shaped particles described herein. 但是,片形颗粒一般具有彼此相对的主表面,这些相对的主表面一般是平整的,且相互平行。 However, platelet-shaped particles generally have opposite major surface each other, the opposing major surfaces being generally planar and parallel to each other. 另外,片形颗粒的特征是其第二纵横比大于针形颗粒的第二纵横比,一般不小于约3 : 1, 例如不小于约6 : 1,或者甚至不小于约10 : 1。 Further, characterized in that platelet-shaped particles it is a second aspect ratio is greater than a second aspect ratio of needle-shaped particles, generally not less than about 3: 1, such as not less than about 6: 1, or even not less than about 10: 1. 通常,垂直于相对的主表面或面的最短维度或边缘维度一般小于50纳米。 Typically, the shortest dimension or edge dimension perpendicular to the opposite major surfaces or faces, is generally less than 50 nanometers.

[0022] 勃姆石微粒材料的形态可以进一步用粒度、更具体地用平均粒度来定义。 [0022] of Stone boehmite particulate material may be further treated with the particle size, average particle size and more specifically defined. 这里,引晶勃姆石微粒材料,即通过引晶处理(下文中将详细描述)形成的勃姆石,具有相对较细的粒度或微晶尺寸。 Here, the seeded boehmite particulate material, that is, by seeding process (described in detail hereinafter) formed boehmite, having a relatively fine particle or crystallite size. 一般而言,平均粒度不大于约1000纳米,在约100至1000纳米的范围内。 In general, the average particle size of not greater than about 1000 nanometers, in the range of about 100 to 1000 nanometers. 其它实施方式具有更细的平均粒度,例如不大于约800纳米、600纳米、500纳米、400纳米, 甚至颗粒的平均粒度小于300纳米,代表一种细微粒材料。 Other embodiments having a finer mean particle size, such as not greater than about 800 nanometers, 600 nanometers, 500 nanometers, 400 nanometers, and even particles smaller than the average particle size of 300 nanometers, representing a finely divided particulate material.

[0023] 文中所用的术语“平均粒度”用来表示颗粒的最长维度或长度的平均值。 [0023] As used herein, the term "average particle size" is used to denote the average longest or length dimension of the particles. 因为颗粒是细长形态,常规的表征技术一般不足以测量平均粒度,因为表征技术通常基于假设颗粒是球形的或近球形。 Because the particles are elongated morphology, conventional characterization technology is generally inadequate to measure average particle size, since characterization technology is generally based on the assumption particles are spherical or nearly spherical. 因此,通过选择多个代表性样品并物理地测量这些代表样品的粒度来确定平均粒度。 Thus, the average particle size is determined by selecting a plurality of representative samples and physically measuring the particle sizes of a representative sample of these. 这类样品可通过各种不同的表征技术如扫描电子显微镜(SEM)来进行选择。 Such samples may be selected as a scanning electron microscope (SEM) by various characterization techniques.

[0024] 研究发现,本发明的引晶勃姆石微粒材料具有细小的平均粒度,而常与之竞争的基于非引晶处理(non-seeded)的技术一般不能提供这样细小的平均粒度。 [0024] found that the present invention is seeded boehmite particulate material having a fine average particle size, and often competing non-seeded based processing (non-seeded) techniques generally can not provide such a fine average particle size. 就此而言,要注意,通常在文献中所报导的粒度不是以本说明书中同样的平均值来陈述的,而是描述为通过物理检测微粒材料样品得到的粒度标称范围。 In this regard, it is noted, is typically reported in the literature are not the same average particle size in this specification to set forth, but is described as a nominal range of particle sizes obtained by detecting a physical sample of the particulate material. 因此,平均粒度将落在现有技术中所报导的范围内,对于预期的高斯粒度分布,一般约在报导范围的算术中点。 Accordingly, the average particle size will fall within the prior art reported in the range, for the expected Gaussian particle size distribution, typically at about the arithmetic midpoint of the reported range. 或者换而言之,虽然基于非引晶处理技术会报导细粒度,但是这种细小尺寸一般指所观测的粒度的下限值,而不是平均粒度值。 Or in other words, although the non-seeded based technologies may report fine grain processing, but such fine size generally refers to the lower limit of an observed particle size, rather than the average particle size values.

[0025] 同样,以类似的方式,以上报导的纵横比一般对应于由代表性样品得到的平均纵横比,而不是与微粒材料纵横比相关联的上限或下限值。 [0025] Likewise, in a similar manner, the aspect ratio reported above generally correspond to the average aspect ratio obtained from representative samples of the particulate material rather than upper or lower limit of the aspect ratio associated. 通常在文献中报导的颗粒纵横比不是以本说明书同样的平均值来陈述的,而是描述为通过物理检测微粒样品得到的纵横比标称范围。 A commonly reported in the literature particle aspect ratios are not the same in the present specification to set forth the average value, but is described as being obtained by detecting a physical aspect ratio of the nominal range of particle samples. 因此,平均纵横比将落在现有技术中所报导的范围内,对于预期的高斯颗粒形态分布,一般约在报导范围的算术中点。 Accordingly, the average aspect ratio will fall within the prior art reported in the range, for the expected Gaussian particle morphology distribution, typically at about the arithmetic midpoint of the reported range. 或者换而言之,基于非引晶处理的技术会报导纵横比,但是这种数据一般是指观测到的纵横比分布的下限值,而不是平均纵横比值。 Or in other words, based on the non-seeded technical process will report aspect ratio, such data generally refers but the observed lower limit of the aspect ratio distribution and not average aspect ratio.

[0026] 除了微粒材料的纵横比和平均粒度外,可以进一步根据比表面积来表征微粒材料的形态。 [0026] In addition to aspect ratio and average particle size of the particulate material, the specific surface area may be further characterized according to the morphology of the particulate material. 这里,使用贯常可用的BET技术来测量微粒材料的比表面积。 Here, penetration often available BET technique to measure the specific surface area of ​​the particulate material. 依据文中所述的实施方式,勃姆石微粒材料具有较高的比表面积,通常不小于约10平方米/克,例如不小于约50平方米/克、70平方米/克或不小于约90平方米/克。 According to embodiments described herein, the boehmite particulate material having a high specific surface area, generally not less than about 10 m2 / g, such as not less than about 50 m2 / g, 70 m2 / g or not less than about 90 m / g. 因为比表面积随颗粒形态及粒度而变,所以诸实施方式的比表面积一般小于约400平方米/克,例如小于约350或300平方米/克。 Because the specific surface area with particle morphology and particle size becomes, the specific surface area of ​​the various embodiments was less than about 400 m / g, such as less than about 350 or 300 m / g.

[0027] 再来详细讨论可用来制造勃姆石微粒材料的方法,大致椭球形、针形或片形的勃姆石颗粒用勃姆石前体(通常是包括铝土矿物在内的含铝材料)经过热液处理而形成,如在上述共有的美国专利4797139中所述的。 [0027] The method discussed in detail again used to produce boehmite particulate material, substantially ellipsoid, needle, or platelet-shaped boehmite particles of the boehmite precursor (typically including bauxite composition including aluminum material) formed after the hydrothermal treatment, as described in the commonly owned U.S. Patent No. 4,797,139. 更具体地,勃姆石微粒材料可通过以下步骤形成:将勃姆石前体与勃姆石晶种在悬浮液中混合,使该悬浮液(或者溶胶或浆料)接受热处理,促使原料转化为勃姆石微粒材料,此外受到悬浮液中提供的勃姆石晶种的影响。 More specifically, the boehmite particulate material may be formed by the following steps: combining the boehmite precursor and boehmite seeds in suspension mixing, the suspension (alternatively sol or slurry) to heat treatment to cause conversion of the feedstock is a boehmite particulate material, in addition influenced boehmite seeds provided in suspension thereof. 加热一般在自生环境即高压釜中进行,因此在该过程中压力升高。 Heating is generally carried out in an autogenous environment, i.e. in the autoclave, the pressure increases in the process. 悬浮液的PH值通常选择在小于7或大于8的数值,勃姆石晶种材料的粒度小于约0. 5微米。 PH value of the suspension is generally selected from a value less than 7 or greater than 8, and the boehmite seed material particle size is less than about 0.5 microns. 一般而言,本发明中晶种颗粒的量大于勃姆石前体的1重量% (以Al2O3计算)。 Generally, the amount of the seed particles of the present invention in front boehmite body 1 wt% (calculated as Al2O3). 加热在约120°C、例如大于约125°C、 或者甚至大于约130°C的温度,大于约85psi、例如大于约90psi、100psi、或者甚至大于约IlOpsi的压力下进行。 Heated at about 120 ° C, e.g., greater than about 125 ° C, or even greater than about 130 ° C a temperature greater than about 85 psi, such as greater than about 90psi, 100psi, or even greater than about IlOpsi performed at a pressure.

[0028] 可以在长时间热液环境再结合较低晶种量和酸性pH值的条件下制造微粒材料, 结果使勃姆石沿着一个晶轴或两个晶轴优先生长。 [0028] The particulate material may be manufactured under hydrothermal conditions for a long time environment combined with relatively low seeding amount and acidic pH, resulting in preferential growth of boehmite along one axis or two crystal axes of the crystal. 一般来说,较长时间的热液处理可以用来生产较长、纵横比较高的勃姆石颗粒和/或总体较大的颗粒。 Generally, the longer the hydrothermal treatment may be used to produce long, high aspect ratio of the boehmite particles and / or larger particles in general.

[0029] 在热处理(例如通过热液处理)和勃姆石转化后,一般通过例如超滤法或通过热处理蒸发剩余液体来除去液体物质。 [0029] In a heat treatment (e.g., by hydrothermal treatment) the stone and boehmite conversion, the liquid material is generally removed by, for example ultrafiltration or evaporation of the remaining liquid by a heat treatment. 在此之后,一般将所得物质碾碎,例如达到100目。 After that, the resultant mass was crushed in general, for example, up to 100 mesh. 要注意,这里所述的微粒粒度一般描述的是通过处理形成的单个微晶,而不是留在某些实施方式中的聚集体(例如,那些称为聚集材料的产物)。 It is noted that the particulate size described herein generally describes the single crystallites formed through processing, rather than remain in certain embodiments, aggregates (e.g., those referred to as aggregate material in the product).

[0030] 根据本发明人收集的数据,可以在处理勃姆石原料的过程中对一些变量作一些调整,以实现所需的形态。 [0030] According to the present invention, the data collected, some variables may make some adjustments during the processing of the boehmite raw material, to achieve the desired shape. 这些变量令人瞩目地包括重量比即勃姆石前体与勃姆石晶种的比例、处理过程中所用酸或碱的具体类型或种类(以及相对PH值)和体系的温度(其与自生热液环境中的压力成正比)。 These variables include remarkable particular type or kind (PH value and relative) i.e. a weight ratio of boehmite precursor to boehmite seed ratio of acid or base used during processing and the temperature of the system (with autogenic proportional to the pressure of hydrothermal environment).

[0031] 特别地,当改变重量比而保持其它变量不变时,形成勃姆石微粒材料的颗粒的形状和尺寸发生变化。 [0031] In particular, when changing the weight ratio of maintaining other variables constant, the shape and size of the particles forming the boehmite particulate material is changed. 例如,当处理是在180°C、在2重量%的硝酸溶液中、以90 : 10的ΑΤΗ: 勃姆石晶种比例进行2小时,形成针形颗粒(ΑΤΗ是勃姆石前体物质)。 For example, when the process is 180 ° C, in a 2 weight% nitric acid solution to 90: ΑΤΗ 10 is: boehmite seed ratio for 2 hours to form a needle-shaped particles (ΑΤΗ boehmite precursor) . 相反,当ΑΤΗ:勃姆石晶种比例减少到80 : 20时,颗粒的形状变得更接近椭球一些。 In contrast, when ΑΤΗ: boehmite seed ratio is reduced to 80: 20, the particle shape becomes closer to some of the ellipsoid. 而且,当该比例进一步减少到60 : 40时,颗粒变为近球形。 Further, when the ratio is further reduced to 60: 40, the particles become near-spherical. 因此,最典型的是勃姆石前体与勃姆石晶种的比例不小于约60 : 40,例如不小于约70 : 30或80 : 20。 Accordingly, most typically the ratio of boehmite precursor to boehmite seeds is not less than about 60: 40, such as not less than about 70: 30 or 80: 20. 但是,为了确保足够的引晶水平(seedinglevel)以促进形成所需的细微粒形态,勃姆石前体与勃姆石晶种的重量比一般不大于约98 : 2。 However, to ensure adequate seeding levels (seedinglevel) to promote formation of the desired form of fine particles, boehmite precursor to boehmite seeds is generally not greater than the weight ratio of about 98: 2. 根据以上所述,重量比的增加一般伴随纵横比的增大,而重量比的减少一般伴随纵横比的减小。 The increase of the above weight ratio is generally accompanied by an increase in the aspect ratio, while reducing the aspect ratio is generally accompanied by reduced weight.

[0032] 此外,当改变酸或碱的类型而保持其它变量不变时,颗粒的形状(例如,纵横比) 和尺寸也会受到影响。 [0032] Further, when changing the type of acid or base, while maintaining the other variables constant, the shape (e.g., aspect ratio) and size will also be affected. 例如,当处理是在100°C、以ATH :勃姆石晶种为90 : 10的比例、在2 重量%的硝酸溶液中进行时,所合成的颗粒一般是针形的,相反,当硝酸被浓度为1重量% 或小于1重量%的HC1取代时,所合成的颗粒一般是近球形的。 For example, when the process is 100 ° C, to ATH: boehmite seed to 90: Comparative Example 10, when in a 2 weight% nitric acid solution, the synthesized particles are generally needle-shaped, on the contrary, when nitric acid substituent is at a concentration of 1 wt% or less than 1% by weight of HC1, the synthesized particles are generally near spherical. 当使用浓度等于或大于2 重量%的此1时,所合成的颗粒一般变为针形。 When used at a concentration equal to or greater than 2 wt% of this 1, the synthesized particles become generally needle-shaped. 对于1重量%的甲酸,所合成的颗粒是片形的。 For 1 wt% of formic acid, the synthesized particles is platelet-shaped. 此外,使用碱溶液,例如1重量%的1(011,则所合成的颗粒是片形的。如果使用酸和碱的混合物,例如1重量%的K0H和0. 7重量%的硝酸,则所合成颗粒的形态是片形。 Further, an alkali solution, such as 1 wt% of a (011, then the synthesized particles is platelet-shaped in. If a mixture of acids and bases, for example, 1 wt% of K0H and 0.7 wt% nitric acid, then the form of synthetic particles are platelet-shaped.

[0033] 合适的酸和碱包括:无机酸,例如硝酸;有机酸,例如甲酸;含卤酸,例如盐酸;和酸性盐(acidic salt),例如硝酸铝和硫酸镁。 [0033] Suitable acids and bases include: inorganic acids, such as nitric acid; organic acids such as formic acid; halogen-containing acids, such as hydrochloric acid; and an acidic salt (acidic salt), such as aluminum nitrate and magnesium sulfate. 有效的碱包括:例如,胺,包括氨;碱金属氢氧化物,例如氢氧化钾;碱性氢氧化物,例如氢氧化钙;和碱性盐(basic salt)。 Effective bases include: for example, amines including ammonia; alkali metal hydroxides, such as potassium hydroxide; alkali hydroxides, such as calcium hydroxide; and basic salts (basic salt).

[0034] 而且,当改变温度而保持其它变量不变时,粒度通常会发生明显的变化。 [0034] Further, when changing the temperature while maintaining the other variables constant, particle size is typically significantly changed. 例如,当处理是以ATH :勃姆石晶种为90 : 10的比例、在2重量%的硝酸溶液中、在150°C进行两小时,由XRD(X射线衍射表征法)得到晶体尺寸为115埃。 For example, when the process is ATH: boehmite seed 90: 10 ratio, in a 2 weight% nitric acid solution, carried out at 150 ° C for two hours by the XRD (X-ray diffraction characterization) to give a crystal size 115 angstroms. 但是,在160°C处理,平均粒度为143埃。 However, at 160 ° C to an average particle size of 143 Angstroms. 因此,随着温度升高,粒度也增大,表明粒度与温度之间的成正比例关系。 Accordingly, as temperature is increased, particle size is also increased, representing a directly proportional relationship between particle size and temperature.

[0035] 实施例1,片形颗粒的合成 [0035] Example 1, Synthesis of platelet-shaped particles

[0036] 向高压釜中加入7. 42磅从Alcoa购得的Hydral710氢氧化铝、0. 82磅从SAS0L以品名Catapal B假勃姆石购得的勃姆石、66. 5磅去离子水、0. 037磅氢氧化钾和0. 18磅22 重量%的硝酸。 [0036] Add 7.42 lbs Hydral710 purchased from Alcoa aluminum hydroxide to the autoclave, 0.82 lbs to name Catapal B pseudoboehmite SAS0L available from boehmite, 66.5 lbs of deionized water , 0.037 lbs of potassium hydroxide and 0.18 lbs of 22 wt% nitric acid. 先将勃姆石预分散在5磅水和0. 18磅酸中,再加入到氢氧化铝和剩余的水和氢氧化钾中。 The boehmite was pre-dispersed in 5 lbs and 0.18 lbs of water in the acid before adding to the aluminum trihydroxide and the remaining water and potassium hydroxide.

[0037] 在530rpm转速搅拌下,高压釜在45分钟内加热到185°C,并在此温度维持2小时。 [0037] Under stirring speed 530rpm, the autoclave was heated in 45 minutes to 185 ° C, and maintained at this temperature for 2 hours. 自生的压力达到约163psi,并保持在该压力。 Autogenous pressures up to about 163psi, and held at that pressure. 然后,将勃姆石分散体从高压釜中取出。 Then, the boehmite dispersion was removed from the autoclave. 在高压釜处理后,溶胶的pH约为10。 After the autoclave treatment, pH of the sol was about 10. 在65°C除去液体物质。 Liquid content was removed at 65 ° C. 将所得物质碾碎到小于100目。 Resultant mass was crushed to less than 100 mesh. 所得粉末的SSA约为62平方米/克。 SSA of the resultant powder was about 62 m / g.

[0038] 实施例2,针形颗粒的合成 2, needle-shaped particles of Synthesis Example [0038] Embodiment

[0039] 向高压釜中加入250克从Alcoa购得的Hydral710氢氧化铝、25克从SAS0L以品名Catapal B假勃姆石购得的勃姆石、1000克去离子水和34. 7克18%的硝酸。 [0039] Aluminum hydroxide was added 250 g Hydral710 purchased from Alcoa to the autoclave, 25 g to name Catapal B pseudoboehmite SAS0L available from boehmite, 1000 g of deionized water and 34.7 g 18 % nitric acid. 先将勃姆石预分散在100克水和6. 9克的酸中,再加入到氢氧化铝和剩余的水和酸中。 The boehmite was pre-dispersed in 100 g of water and 6.9 g of the acid before adding to the aluminum trihydroxide and the remaining water and acid.

[0040] 在530rpm转速搅拌下,高压釜在45分钟内加热到180°C,并在此温度维持2小时。 [0040] Under stirring speed 530rpm, the autoclave was heated in 45 minutes to 180 ° C, and maintained at this temperature for 2 hours. 自生的压力达到约150psi,并保持在该压力。 Autogenous pressures up to about 150psi, and held at that pressure. 然后,将勃姆石分散体从高压釜中取出。 Then, the boehmite dispersion was removed from the autoclave. 在高压釜处理后,溶胶的pH约为3。 After the autoclave treatment, pH of the sol was about 3. 在95°C除去液体物质。 Liquid content was removed at 95 ° C. 将所得物质碾碎到小于100目。 Resultant mass was crushed to less than 100 mesh. 所得粉末的SSA约为120平方米/克。 SSA of the resultant powder was about 120 m / g.

[0041] 实施例3,椭球形颗粒的合成 Synthesis Example 3 ellipsoidal particles [0041] Embodiment

[0042] 向高压釜中加入220克从Alcoa购得的Hydral710氢氧化铝、55克从SAS0L以品名Catapal B假勃姆石购得的勃姆石、1000克去离子水和21. 4克18%的硝酸。 [0042] Aluminum hydroxide was added 220 g Hydral710 purchased from Alcoa the autoclave 55 grams of Catapal B pseudoboehmite name available from SAS0L boehmite, 1000 g of deionized water and 21.4 g 18 % nitric acid. 先将勃姆石预分散在100克水和15. 3克酸中,再加入到氢氧化铝和剩余的水和酸中。 The boehmite was pre-dispersed in 100 g of water and 15.3 g of the acid before adding to the aluminum trihydroxide and the remaining water and acid. [0043] 在530rpm转速搅拌下,高压釜在45分钟内加热到172°C,并在此温度维持3小时。 [0043] Under stirring speed 530rpm, the autoclave was heated in 45 minutes to 172 ° C, and maintained at this temperature for 3 hours. 自生的压力达到约120psi,并保持在该压力。 Autogenous pressures up to about 120psi, and held at that pressure. 然后,将勃姆石分散体从高压釜中取出。 Then, the boehmite dispersion was removed from the autoclave. 在高压釜处理后,溶胶的PH约为4。 After the autoclave treatment, PH sol is about 4. 在95°C除去液体物质。 Liquid content was removed at 95 ° C. 将所得物质碾碎到小于100目。 Resultant mass was crushed to less than 100 mesh. 所得粉末的SSA约为135平方米/克。 SSA of the resultant powder was about 135 m / g.

[0044] 实施例4,沂球形颗粒的合成 Synthesis Example 4 Yi spherical particles [0044] Embodiment

[0045] 向高压釜中加入165克从Alcoa购得的Hydral710氢氧化铝、110克从SASOL以品名Catapal B假勃姆石购得的勃姆石、1000克去离子水和35. 2克18%的硝酸。 [0045] Aluminum hydroxide was added 165 g Hydral710 purchased from Alcoa to the autoclave, 110 g under the name Catapal B pseudoboehmite available from SASOL boehmite, 1000 g of deionized water and 35.2 g 18 % nitric acid. 先将勃姆石预分散在100克水和30. 6克酸中,再加入到氢氧化铝和剩余的水和酸中。 The boehmite was pre-dispersed in 100 g of water and 30.6 g of the acid before adding to the aluminum trihydroxide and the remaining water and acid.

[0046] 在530rpm转速搅拌下,高压釜在45分钟内加热到160°C,并在此温度维持2. 5小时。 [0046] Under stirring speed 530rpm, the autoclave was heated in 45 minutes to 160 ° C, and maintained at this temperature for 2.5 hours. 自生的压力达到约lOOpsi,并保持在该压力。 Autogenous pressure of about lOOpsi, and maintained at that pressure. 然后,将勃姆石分散体从高压釜中取出。 Then, the boehmite dispersion was removed from the autoclave. 在高压釜处理后,溶胶的PH约为3. 5。 After the autoclave treatment, sol PH of about 3.5. 在95°C除去液体物质。 Liquid content was removed at 95 ° C. 将所得物质碾碎到小于100 目。 Resultant mass was crushed to less than 100 mesh. 所得粉末的SSA约为196平方米/克。 SSA of the resultant powder was about 196 m2 / g.

[0047] 依据文中所述的实施方式,较有效且灵活的方法可用使将最终的勃姆石产物具有所需的形态。 [0047] According to the embodiment described herein, more efficient and flexible method may be used to make the final boehmite product having a desired morphology. 尤其重要的是,所述实施方式使用引晶处理,得到一种高投入产出且可以高度控制处理过程的处理途径,可以最终得到所需的平均粒度和受控制的粒度分布。 Of particular importance is the embodiment using a seeding process, to obtain a high-input-output and the processing route may be highly controlled process, can finally give the desired average particle size and a controlled particle size distribution. 将以下二者组合是特别重要的:(i)确认和控制方法中的关键变量,例如重量比、酸和碱的类型以及温度;和(ii)基于引晶的技术,提供对所需勃姆石微粒材料形态的可重复和可控制的处理。 The following combinations of the two are particularly important: (i) confirmation key variables and control methods, such as weight ratio, acid and base type and temperature; and (ii) seeding-based technology to provide the desired boehmite stone material forms particles repeatable and controllable process.

[0048] 本发明的诸方面使勃姆石微粒材料能够使用在许多应用中,例如专用涂料以及聚合物产品的填料。 [0048] Aspects of the present invention that the boehmite particulate material may be used in many applications, such as fillers and coatings for polymer product. 事实上,可以通过常规的配混方法使微粒材料单独且均勻地分散在溶剂(尤其包括极性溶剂)和/或聚合物中,而不形成聚集体。 Indeed, the particulate material can be made by conventional compounding methods individually and uniformly dispersed in a solvent (in particular, include polar solvents), and / or polymers without forming aggregates. 另外,可以利用常规的分散剂如硅烷偶联剂使勃姆石微粒材料单独且均勻地分散在非进行溶剂和/或聚合物中,而不形成聚集体。 Further, using conventional dispersant such as a silane coupling agent boehmite particulate material individually and uniformly dispersed solvent and / or a non-polymer, without formation of aggregates. 当然,勃姆石微粒材料的具体应用不受限制,可以在商业使用于许多应用中。 Of course, the particular application is not limited stone boehmite particulate material may be used in many commercial applications.

[0049] 虽然在说明实施方式中对本发明进行了说明和描述,但是本发明不受限于这些详细描述,因为在以任何方式背离本发明范围的前提下,可以进行各种修改和替代。 [0049] While the invention has been illustrated and described in the description of embodiments, the present invention is not limited to these described in detail since the premise in any way departing from the scope of the invention, various modifications and substitutions. 例如,可以提供其它或等同的替代物,或者可以使用等同的生产步骤。 For example, it can provide other equivalent or alternative or equivalent production steps can be used. 这样,本领域技术人员可以只使用常规实验对文中所揭示的本发明进行其它变化和等同,所有这些变化和等同据信在所附权利要求所限定的本发明的范围内。 Thus, those skilled in the art can use routine experimentation the present invention herein disclosed that other variations and equivalents within the scope of the present invention all such modifications and equivalents are believed defined in the appended claims.

Claims (9)

  1. 一种形成勃姆石微粒材料的方法,其包括:以悬浮液的形式提供勃姆石前体和勃姆石晶种,勃姆石前体与勃姆石晶种的重量比不小于60∶40;在高于120℃的温度对所述悬浮液进行热处理,以使勃姆石前体转化为勃姆石微粒材料,所述勃姆石微粒材料主要由片形颗粒组成,其纵横比不小于3∶1,并且其第二纵横比不小于3∶1,所述的方法在甲酸、KOH或KOH和硝酸的混合物中进行。 A method for forming boehmite particulate material, comprising: providing a boehmite precursor and boehmite seeds in a suspension of boehmite precursor to boehmite seeds is not less 60:40 weight ratio of 40; at a temperature higher than 120 deg.] C heat treatment of the suspension, so that the boehmite precursor into boehmite particulate material, the boehmite particulate material mainly composed of platelet-shaped particles having an aspect ratio of not less than 3:1, and a second aspect ratio of not less than 3, the method is performed in a mixture of KOH or KOH formic acid and nitric acid.
  2. 2.如权利要求1所述的方法,其特征在于,所述热处理在高于130°C的温度进行。 2. The method according to claim 1, wherein said heat treatment is performed at a temperature of above 130 ° C.
  3. 3.如权利要求1所述的方法,其特征在于,所述热处理在高于85psi的压力下进行。 The method according to claim 1, characterized in that the heat treatment is carried out at a pressure above 85psi.
  4. 4.如权利要求1所述的方法,其特征在于,所述重量比不小于80 : 20。 4. The method according to claim 1, wherein the weight ratio is not less than 80: 20.
  5. 5.如权利要求4所述的方法,其特征在于,所述勃姆石前体与勃姆石晶种的重量比不大于98 : 2。 5. The method according to claim 4, wherein the boehmite precursor to boehmite seeds is not greater than the weight ratio of 98: 2.
  6. 6.如权利要求1所述的方法,其特征在于,所述勃姆石微粒材料的平均粒度不大于1000纳米。 6. The method according to claim 1, wherein an average particle size of the boehmite particulate material is not greater than 1000 nm.
  7. 7.如权利要求1所述的方法,还包括设置下列条件中的至少一个以使勃姆石微粒材料的平均粒度不大于1000纳米:热处理温度、或勃姆石前体与勃姆石晶种的重量比。 7. The method according to claim 1, further comprising setting at least one of the following conditions that the boehmite particulate material to an average particle size not greater than 1000 nm: heat treatment temperature, or boehmite precursor and boehmite seeds the weight ratio.
  8. 8.如权利要求7所述的方法,其特征在于,提高勃姆石前体与勃姆石晶种的比例以增大纵横比,或者降低所述比例以减小纵横比。 8. The method according to claim 7, characterized in that, to increase the proportion of boehmite precursor to boehmite seeds to increase the aspect ratio, or decreased to reduce the ratio of the aspect ratio.
  9. 9.如权利要求7所述的方法,其特征在于,提高热处理温度以增大粒度,或者降低热处理温度以减小粒度。 9. The method according to claim 7, wherein the heat-treating temperature in order to increase particle size, or reducing the temperature of the heat treatment to reduce particle size.
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